Dimethylamine → Dimethyl-[2-(3-nitro-benzenesulfonyl)-ethyl]-amine

HRID 1957978ノート

反応式

HRID 1957978 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([S:10]([CH2:13][CH2:14]O)(=[O:12])=[O:11])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[CH3:16][NH:17][CH3:18]>C(O)C.ClCCl>[CH3:16][N:17]([CH3:18])[CH2:14][CH2:13][S:10]([C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)(=[O:12])=[O:11]

参加物

5

反応物 2

HCID 674DimethylamineHCID 170561Ethanol, 2-[(3-nitrophenyl)sulfonyl]-

生成物 1

HCID 68425174Dimethyl-[2-(3-nitro-benzenesulfonyl)-ethyl]-amine収率 59.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

実験手順

2-(3-Nitro-phenylsulfonyl)-ethanol (0.5 g; 2.6 mmol) was dissolved in 3 mL ethanol and 2 mL of dichloromethane. Then 1 mL of (7.8 mmol) dimethylamine (33% in ethanol) was added, the reaction mixture was subsequently concentrated in vacuo, dissolved in dichloromethane, and the product was precipitated by adding diethyl ether and petrol ether. 0.4 g (1.55 mmol; 59% yield) of dimethyl-[2-(3-nitro-benzenesulfonyl)-ethyl]-amine were obtained as a yellow solid.

後処理

  1. concentrationthe reaction mixture was subsequently concentrated in vacuo
  2. dissolutiondissolved in dichloromethane
  3. customthe product was precipitated
  4. additionby adding diethyl ether and petrol ether

出典と根拠

ORDレコード
ord-201a381533a24327bfc9497915fbee9a
出典データセット
uspto-grants-2013_04
特許番号
US08410100B2

反応ノート

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